JP2658146B2 - Chromatographic spectrometer connection device - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to an interface for connecting a chromatograph to a spectroscopic analyzer.

(Prior art) When analyzing a sample component separated by chromatography by spectroscopic means, the fluid flowing out of the chromatographic column is guided to a flow cell, measurement light is incident on the flow cell, and measurement light transmitted through the flow cell is transmitted to the flow cell. Perform photometry. In gas chromatography, packed columns and capillary columns are used depending on the purpose of analysis.However, these columns have different thicknesses, and when connecting other devices to these columns, use a common connector. Can not. However, conventional general-purpose spectrometers are equipped with a flow cell for performing measurement using a flow cell and a connector for connecting the flow cell to a predetermined tubing as an accessory device, but the types of columns that can be connected are limited. In particular, it was difficult to exchange different types of columns such as packed columns and capillary columns.

(Problem to be Solved by the Invention) By providing a versatility to a connector portion for connecting a flow cell, which is an interface between the chromatograph and the spectroscopic analyzer, for connecting the chromatograph to a pipe system of the chromatograph,
In order to connect the flow cell easily even if the column is exchanged between different types of columns such as packed column and capillary column in the chromatograph, and to suppress the performance degradation due to column connection It is another object of the present invention to provide a device having a secondary advantage that a makeup gas flow path for mixing can be secured.

(Means for Solving the Problems) A conducting tube into which a sample of a flow cell flows is branched, and a large-diameter connector for a packed column is attached to one branch end, and a capillary-column connector for a capillary column is attached to the other branch end. A small-diameter connector is attached, the gas outlet pipe of the makeup gas supply means is branched, and a flow control valve is interposed in each branch, and a connector compatible with the large-diameter connector is connected to one branch end at the other branch. At the end, attach a connector that fits the small diameter connector.When a packed column is connected to the flow cell, make up the connector through the connector that fits the small diameter connector at the free branch end of the free end of the flow tube. When the gas supply means is connected and the capillary column is connected to the flow tube of the flow cell, it is suitable for the large diameter connector at the free branch end The makeup gas supply means is connected via a connector.

(Operation) As described above, the packed column and the capillary column have different thicknesses, and cannot be connected to the flow cell with a common connector. According to the present invention, at least one of the conduits into which the sample of the flow cell flows in and out is branched,
Since different size connectors are connected to the branch ends, a large-diameter connector is used for a packed column, and a small-diameter connector is used for a capillary column. Can be connected. In this case, the branch end without connecting the column is not simply closed, but also used as a makeup gas supply pipe required for connecting the column, thereby eliminating the adverse effect of dead space generated inside the flow path. Can be.

By branching both of the conduits at both ends of the flow cell and attaching large-diameter and small-diameter connectors, respectively, the sample can flow from either end of the flow cell, which is more convenient.

(Embodiment) FIG. 1 shows an embodiment of the present invention. Reference numeral 1 denotes a gas chromatograph oven having a built-in chromatographic column. Reference numeral 2 denotes a sample vaporization chamber to which a column is connected. As a column, either a packed column or a capillary column can be connected. A carrier gas source 4 is externally connected to the sample vaporization chamber via a flow control valve 5, an electromagnetic valve 6, and a filter 7, and the carrier gas flows from the sample vaporization chamber to the column. The sample is injected into the sample vaporization chamber 2 by a micro syringe.
The oven 1 is provided with a packed column connection connector 8 and a capillary column connection connector 9.
The packed column is connected between the sample vaporization chamber 2 and the packed column connection connector 8. In the case of a capillary column, the sample vaporization chamber 2 and the connector 9 for connecting the capillary column
Connected between 1 shows the case where the packed column 3p is connected, and the dotted line shows the case where the capillary column 3c is connected. Numeral 10 denotes a light pipe, which is a flow cell for allowing measurement light to pass in the direction of the tube axis. Conductive tubes 10b and 10c are connected to both side surfaces of the light pipe 10, and the conductive tube 10b is branched by a T-shaped tube, and the branch end of the T-shaped branch is connected to a large-diameter connector 8 for a packed column. The straight end is connected to a small-diameter connector 12 for a capillary column. The conduction tube 10c is also branched by a T-shaped tube, and the straight branching end is connected to the capillary column connector 9, and the other T-shaped branching end is a large-diameter connector 13 for packed column connection. It is connected to the. Reference numeral 18 denotes a connector for connecting a detector. The gas flowing out of the column is passed through the light pipe 10, and the measurement light is passed through the window 10a in the tube axis direction. The measuring light passes through the light pipe while repeating reflection. When the packed column is used in the above-described configuration, the column 3p is connected between the sample vaporization chamber 2 and the connector 8 as shown by the solid line in FIG. It flows out of the side and flows through the connector 9 to the detector connected to the connector 18. The connectors 12 and 13 are connected to a makeup gas source 14, and a flow rate control valve 16 and a pressure gauge 17 are respectively provided in the middle of the flow path. The makeup gas sent to the conduits 10b and 10c via the connectors 12 and 13 remains as the sample component flows into the dead space between the connectors 12 and 13 and the conduits 10b and 10c, and remains at the bottom of the chromatogram peak. It is intended to prevent the ghost from appearing in the analysis result by subtracting the value from the sample or mixing with the sample component coming later.

When a capillary column is used, the capillary column 3c is connected between the sample vaporization chamber 2 and the connector 9 as shown by a dotted line in FIG. FIG. 2 shows the pipe connection in this case. The gas flowing out of the column flows into the light pipe from the right end of the light pipe 10, flows out from the left end, and reaches the detector through the connector 18. In this case, the connector 8 is connected to the makeup gas source 14, and the sample component is prevented from flowing into and remaining in the dead space from the connector 8 to the conduction interval 10b.

3A and 3B show details of the conduits 10b and 10c. Conduit 10b,
10c has a straight end connected to a small-diameter connector 12 or 9 for a capillary, and a T-shaped end connected to a large-diameter connector 8 or 13 for a packed column. ing. When connecting a capillary column, refer to Fig. 3A
Connect the end of the capillary column 3c to the light pipe 10 as shown in
Then, it is inserted into the inner surface of the wall to the opening to the conduction tube, fixed with a connector, and makeup gas is sent from the T-shaped branched conduction tube. When connecting the packed column, as shown in FIG. 3B, the end of the packed column 3p is inserted and fixed to a large-diameter connector for the packed column. At this time, the makeup gas is sent from the makeup gas source to the capillary connector to the straight portion of the conduit by the capillary, and the capillary is inserted and fixed below the branch portion of the conduit.

In the above description, the column effluent gas passing through the light pipe flows to the detector via the connector 18.
This is because the sample is not subjected to deterioration such as in a detector due to a hydrogen flame or the like only by being subjected to light irradiation while passing through the light pipe and being subjected to the measurement of the absorbance, so that it can be analyzed by another analysis means after the absorbance measurement. In this case, if the diameter of the flow path from the light pipe to the next analysis means is large, the diffusion cross section between the separated sample component and the carrier gas is large, and the mixing of both proceeds, so that the peak of the sample component becomes dull in the next analysis. Therefore, it is desirable that the path from the light pipe to the next analysis means is narrow and short, and a capillary is used for the flow path. Therefore, even when using packed columns, the light pipe
The gas flowing out of 10 is sent to the next detector through the capillary connector 9. The connector 13 is provided in case that connection between the sample vaporization chamber 2 and the connector 13 is easier to connect depending on the packed column. In this case, the sample flows from the connector 13 through the light pipe to the left, From 12 the capillary passes through the connector 18 to the next detector. And the makeup gas is connector 8
And 9.

A mass spectrometer can be used as a means for further analyzing the sample that has passed through the light pipe 10.

FIG. 4 shows another embodiment of the present invention. This embodiment eliminates the branch of the conduit 10c and the connector 13 in the previous embodiment. When a packed column is used, the column is connected between the sample vaporization chamber 2 and the connector 8 as shown by a solid line, From the right end of the light pipe 10 via the connector 9 to the next detector by capillary. At this time, the makeup gas is supplied to the connector 12. When using a capillary column, the column is connected between the sample vaporization chamber 2 and the connector 9 as shown by the dotted line, the sample flows through the light pipe from right to left, through the connector 12 to the next detector, The makeup gas is supplied to the connector 8.

(Effect of the Invention) According to the present invention, since two types of connectors are attached to the flow tube of the flow cell, even if the type of the packed column or the capillary column is different, the flow cell can be connected by either connector. At this time, the makeup gas supply means is connected by the connector that is not used at this time, so there is no danger of dead space formation, and it is possible to easily respond to the exchange of columns in the connection between the chromatograph and the spectrometer. it can.

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view of an essential part of one embodiment of the present invention, FIG. 2 is a flow path connection diagram when a capillary column is used in the above embodiment, and FIG. 3A is a case where a capillary column is connected to a vent pipe. FIG. 3B is an enlarged vertical cross-sectional view when a packed column is connected to a vent pipe, and FIG. 4 is a flow path connection diagram of another embodiment of the present invention. 1 ... gas chromatograph oven, 2 ... sample vaporization chamber, 3p ... packed column, 3c ... capillary column,
4 ... Carrier gas source, 8,13 ... Packed column connector, 10 ... Light pipe, 10b, 10c ... Vent pipe, 1
1… Heating block, 9,12… Connector for capillary connection, 14… Makeup gas source.

Claims (1)

(57) [Claims] 1. A conducting tube through which a sample of a spectroscopic analysis flow cell flows is branched, and a large-diameter connector for a packed column is attached at one branch end, and a small-diameter connector for a capillary column is mounted at the other branch end. A make-up gas supply means is provided, the make-up gas supply pipe of this means is branched into two, and each of the branch pipes has a flow control valve interposed therebetween. Attach a connector compatible with the connector and a connector compatible with the small diameter connector at the other branch end.When using a packed column, connect the packed column to the flow cell with the large diameter connector of the flow tube of the flow cell. Make-up gas is supplied to the small-diameter connector of the conducting tube via the connector that is adapted to the small-diameter connector. A chromatographic spectroscopic analyzer connection device, wherein the capillary column is connected to the flow cell via the small-diameter connector, and the large-diameter connector is supplied with a makeup gas via the connector adapted thereto. .